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Hexane → HCID 10758603、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hexane | HCID 8058 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | 4-methoxy-2-methyl-1H-indole | HCID 10773274 | — |
| 反応物 | 3-(Chloromethyl)-1,1'-biphenyl | HCID 15480892 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | HCID 10758603 | HCID 10758603 | 76.4% |
反応手順
805 mg (5 mmol) of 4-methoxy-2-methyl-1H-indole is reacted with 200 mg (5 mmol) of 60% NaH/mineral oil (washing with hexane before adding DMF) in 15 mL of DMF and after stirring for 0.5 hour, 1.0 g (5 mmol) of 3-(chloromethyl)biphenyl is added. The mixture is stirred at room temperature for 18 hours, diluted with water and extracted with ethyl acetate. The ethyl acetate solution is washed with brine, dried (MgSO4) and after concentrating at reduced pressure, the residue is chromatographed on silica gel eluting with 20% EtOAc/hexane to give 1.25 g (76% yield) of 1-((1,1′-biphenyl)-3-ylmethyl)-2-methyl-4-methoxy-1H-indole mp, 127°-131° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06274616B1 |
| 出典データセット | uspto-grants-2001_08 |
| ORD ID | ord-bdc8da2278f6451085810f4fd9bb8c02 |
| 出典メモ | uspto-grants-2001_08 |